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基于磁铁矿的聚合物负载杂化纳米复合材料的设计与制备:一种在已知钯辅助偶联反应中应用的有前景的多相催化体系。

Design and Fabrication of a Magnetite-based Polymer-supported Hybrid Nanocomposite: A Promising Heterogeneous Catalytic System Utilized in Known Palladium-assisted Coupling Reactions.

机构信息

Catalysts and Organic Synthesis Research Laboratory, Department of Chemistry, Iran University of Science and Technology, Tehran 16846-13114, Iran.

出版信息

Comb Chem High Throughput Screen. 2020;23(2):119-125. doi: 10.2174/1386207323666200128152136.

DOI:10.2174/1386207323666200128152136
PMID:32003667
Abstract

OBJECTIVE

Herein, a novel heterogeneous catalytic system constructed of iron oxide and palladium nanoparticles is presented. Firstly, a convenient synthetic pathway for the preparation of this catalytic system is introduced, then the application of the fabricated nanocomposite in the Pd-catalyzed C─C coupling reactions is monitored. High reaction yields (98%) have been obtained in short reaction time, by using this catalytic system.

MATERIALS AND METHODS

Fe3O4/P4VP-Pd catalytic system was fabricated via an in situ method by 4- vinylpyridine (4-VP). In this regard, all the essential structural analyses such as FT-IR, EDX, VSM, and TGA have been performed on the Fe3O4/P4VP-Pd catalytic system to investigate its properties. The spherical morphology of the NPs and their uniform size have also been studied by the SEM method. Further, the reaction progress was controlled by thin-layer chromatography. Finally, NMR analysis was used to identify the synthesized biphenyl pharmaceutical derivatives.

RESULTS

High efficiency of this catalytic system has been precisely investigated and the optimal conditions were determined. The catalytic process is carried out in 20 min, under mild conditions (room temperature). Then, the purification process is easily performed via magnetic separation of the catalyst NPs. After completion of the synthesis reaction, the NPs were collected, washed, and reused several times.

CONCLUSION

Among recently reported heterogeneous catalytic systems, Fe3O4/P4VP-Pd is recommended due to its high catalytic performance, convenience of the preparation process, excellent biocompatibility, economic benefits, and well reusability. Overall, in order to save time in the complex synthetic processes and also prevent using so many chemical reagents and solvents for the purification process, the presented catalytic system could be suitable for scaling up and applying for the industrial applications.

摘要

目的

本文构建了一种新型的氧化铁和钯纳米粒子的多相催化体系。首先,介绍了该催化体系的一种简便合成方法,然后监测了所制备的纳米复合材料在钯催化的 C─C 偶联反应中的应用。使用该催化体系,在短反应时间内得到了高的反应收率(98%)。

材料和方法

通过 4-乙烯基吡啶(4-VP)的原位方法制备了 Fe3O4/P4VP-Pd 催化体系。在这方面,对 Fe3O4/P4VP-Pd 催化体系进行了所有必要的结构分析,如 FT-IR、EDX、VSM 和 TGA,以研究其性质。还通过 SEM 方法研究了 NPs 的球形形态及其均匀的尺寸。此外,通过薄层色谱法控制反应进度。最后,用 NMR 分析来鉴定合成的联苯药物衍生物。

结果

精确研究了该催化体系的高效率,并确定了最佳条件。在温和的条件(室温)下,催化过程在 20 分钟内进行。然后,通过磁性分离催化剂 NPs 可以很容易地进行纯化过程。合成反应完成后,收集、洗涤并多次重复使用 NPs。

结论

在最近报道的多相催化体系中,由于其高催化性能、制备过程的便利性、优异的生物相容性、经济效益和良好的可重复使用性,推荐使用 Fe3O4/P4VP-Pd。总的来说,为了节省复杂合成过程中的时间,并防止使用如此多的化学试剂和溶剂进行纯化过程,所提出的催化体系可以适用于放大和工业应用。

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